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Rapid preparing method of large-specific-surface-area SAPO-34 molecular sieve

A SAPO-34 technology with large specific surface area, applied in the direction of molecular sieve catalyst, molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, etc. Small particle thickness, reducing the effect of carbon deposition reaction

Active Publication Date: 2019-11-05
SINOCHEM QUANZHOU ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problem that the synthesis period of SAPO-34 molecular sieve is long, the present invention proposes a rapid preparation method of SAPO-34 molecular sieve with large specific surface area

Method used

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  • Rapid preparing method of large-specific-surface-area SAPO-34 molecular sieve
  • Rapid preparing method of large-specific-surface-area SAPO-34 molecular sieve
  • Rapid preparing method of large-specific-surface-area SAPO-34 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0026] Al in product 2 O 3 , P 2 O 5 , SiO 2 , TEAOH, H 2 The molar ratio of O and glycerol is 1:2:0.6:4:140:15. Weigh 4.085g aluminum isopropoxide, 4.6118g phosphoric acid, 1.2000g silica sol, 16.8297g TEAOH, 12.0494g deionized water, 13.9530g glycerol. Dissolve TEAOH in deionized water, slowly add aluminum isopropoxide, stir at room temperature for 1-5 h until the solution is clear; then add silica sol and phosphoric acid under stirring conditions, and react for 2 hours respectively, and finally add glycerol and stir for aging 3d; Then transfer the mixture to a stainless steel kettle with a PTFE liner, and place it in an oven at 180 ℃ to crystallize for 4 hours. Take out centrifugation (8000r / min) and separate for 30min, then wash with water until the pH is lower than 9, and then dry at 110 ℃, and finally put it in a muffle furnace, roast at 550 ℃ for 5 h, remove the organic template, and get the target product (S1).

Embodiment 2

[0028] Al in product 2 O 3 , P 2 O 5 , SiO 2 , TEAOH, H 2 The molar ratio of O to ethylene glycol is 1:2:0.6:4:140:15. Weigh 4.085g aluminum isopropoxide, 4.6118g phosphoric acid, 1.2000g silica sol, 16.8297g TEAOH, 12.1262g deionized water, 9.4042g ethylene glycol. Dissolve TEAOH in deionized water, slowly add aluminum isopropoxide, stir at room temperature for 1-5 h until the solution is clear; then add silica sol and phosphoric acid under stirring conditions, and react for 2 hours respectively, and finally add ethylene glycol and stir for aging 3d; Then transfer the mixture to a stainless steel kettle with a PTFE lining, and place it in an oven at 200 ℃ to crystallize for 4 h. Take out centrifugation (8000r / min) and separate for 30min, then wash with water until the pH is lower than 9, and then dry at 110 ℃, and finally put it in a muffle furnace, roast at 500 ℃ for 6 h, remove the organic template, and get the target product (S2).

Embodiment 3

[0030] Al in product 2 O 3 , P 2 O 5 , SiO 2 , TEAOH, H 2 The molar ratio of O and isopropanol is 1:2:0.6:4:140:15. Weigh 4.085g aluminum isopropoxide, 4.6118gg phosphoric acid, 1.2000g silica sol, 16.8297g TEAOH, 12.0979g deionized water, 9.1015g isopropanol. Dissolve TEAOH in deionized water, slowly add aluminum isopropoxide, stir at room temperature for 1-5 h until the solution is clear; then add silica sol and phosphoric acid under stirring conditions, and react for 2 hours respectively, and finally add isopropanol and stir for aging 3d; Then transfer the mixture to a stainless steel kettle with a PTFE lining, and place it in an oven at 180 ℃ to crystallize for 4 hours. Take out centrifugation (8000r / min) and separate for 30min, then wash with water until the pH is lower than 9, and then dry at 110 ℃, and finally put it in a muffle furnace, roast at 550 ℃ for 5 h, remove the organic template, and get the target product (S3).

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Abstract

The invention discloses a rapid preparing method of a large-specific-surface-area SAPO-34 molecular sieve. The molecular sieve is obtained with an aluminum source, a phosphorus source, a silicon source, a template TEAOH, deionized water and glycerol as the raw materials through crystallization for 4-16 hours at 160-200 DEG C. The introduced glycerol and water in synthesis liquid can form hydrogenbonds, and therefore the content of water in the synthesis liquid is reduced, the saturability of a solution is increased, the rapid nucleation of crystal nucleuses is promoted, the growth of the crystal nucleuses in the later period is facilitated, and the size of particles of the molecular sieve is reduced. Meanwhile, a hydroxyl group in the glycerol and a primary structural unit in the synthesis liquid can have a covalent bonding reaction, the adsorption of the primary structural unit to the surface of the glycerol is promoted, the growth rate of the crystal nucleuses is increased, the required crystallization time is shortened, and thus the preparing cycle of the SAPO-34 molecular sieve can be obviously shortened.

Description

Technical field [0001] The invention belongs to the field of catalyst preparation, and specifically relates to a rapid preparation method of SAPO-34 molecular sieve with large specific surface area. Background technique [0002] At present, the main method for synthesizing SAPO-34 is hydrothermal synthesis, which uses water as the solvent and is carried out in a closed autoclave. The aging time is generally 1-4d, and the crystallization time is 1-3d, and the synthesis cycle is longer. The problem. Among them, the length of the crystallization time will affect the morphology and separation performance of the molecular sieve. If the crystallization time is too short, the reaction is not complete, and there will be amorphous substances in the resulting molecular sieve, which will affect its separation performance; if the crystallization time is too long, the molecular sieve particles may agglomerate and reduce their specific surface area, thereby affecting their separation performa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01J29/85B01J35/10
CPCC01B37/08C01B39/54B01J29/85C01P2006/12B01J35/617Y02P30/40
Inventor 肖文灿范文青张黎徐琳刘长坤
Owner SINOCHEM QUANZHOU ENERGY TECH CO LTD
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